Реакция #53612

Уравнение реакции

Sodium hydride

compound ( 33 )

2,9-Dihydro-6-oxa-2-azabenzo[cd]azulen-8-one ethylene ketal

benzenesulfonyl chloride

→

titled compound ( 34 )

Выход 69.0%

2-Benzenesulfonyl-2,9-dihydro-6-oxa-2-azabenzo[cd]azulen-8-one ethylene ketal

Выход 69.0%

Растворители

dimethylformamide

chloroform hexane

Условия реакции

Обработка

1. 1
   Температураwith cooling in ice
2. 2
   Экстракцияwas extracted with ethyl acetate
3. 3
   ПромывкаThe extracts were washed with brine
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   Концентрированиеconcentrated under reduced pressure
6. 6
   ДругоеThe residue obtained

Методика

60% Sodium hydride 33 mg was added to a solution of compound (33) in dry dimethylformamide 2 ml with cooling in ice and the mixture was stirred for 10 min. Then, benzenesulfonyl chloride 152 mg was added. The mixture was heated at 60° C. for 14 h. Ice-water was added to the reaction mixtures, which was extracted with ethyl acetate. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was choromatographed on aluminum oxide in chloroform:hexane (1:1) to give the titled compound (34) as a pale yellow oil, 187 mg. Yield 69%.

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